Spectrophotometric Determination of Carvone in Caraway Fruits and Essential Oil: Development and Validation of an Analytical Procedure

INTRODUCTION. Caraway fruits are used in the treatment of irritable bowel syndrome and dyspeptic disorders due to their pronounced antispasmodic, antimicrobial, and carminative effects. The antispasmodic activity of caraway seeds isprimarily due to their essential oil content, with carvone being the predominant component. The European Pharmacopoeia 11th edition regulates the carvone content in essential oils, while the State Pharmacopoeia of the Russian Federation XIV edition does not standardize caraway fruits based on their carvone content.
AIM. To develop and validate a spectrophotometric method for the quantification of carvone in the essential oil of caraway fruits and to verify the results of the spectrophotometric determination using gas chromatography — mass spectrometry.
MATERIALS AND METHODS. The study utilized caraway fruits (Carum carvi L.) manufactured by Firma Zdorovie LLC (batch 031224; expiry November, 2027), a carvone reference standard with a purity of 98.5% (Fluka), a UNICO 2802 spectrophotometer (United Products & Instruments, Inc.), ADV-200M analytical balance (GOSMETR), and a GC-MS QP2010 Ultra gas chromatograph (Shimadzu) coupled with a mass-selective detector. For spectrophotometric analysis, aliquots of the essential oil and the carvone reference standard were dissolved in ethanol, 95% (v/v). The absorbance of the solutions was measured at a wavelength of 236 nm in 10 mm path length cells. The results obtained by the spectrophotometric method were confirmed using gas chromatography.
RESULTS. Validation of the spectrophotometric method for the quantitative
determination of carvone, carried out in accordance with the requirements of
OFS.1.1.0012 “Validation of analytical methods” of the State Pharmacopoeia of
the Russian Federation, XV ed., showed its specificity, linearity, precision, and accuracy. The results are not affected by systematic error. The relative standard deviation (RSD) value does not exceed 2.0%. The results of the spectrophotometric determination of carvone (75.7±0.9%) correlate with the results of the gas-liquid chromatography analysis (75.2±0.8%).

CONCLUSIONS. The developed analytical procedure for the quantitative determination of carvone can be employed for the standardization of caraway fruits by introducing an additional quality parameter for their essential oil in the “Assay” section. It is also suitable for the standardization of caraway essential oil when used as a substance for the manufacture of medicinal products.

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